JP2948973B2 - Molded body for thermal history detection - Google Patents
Molded body for thermal history detectionInfo
- Publication number
- JP2948973B2 JP2948973B2 JP4041622A JP4162292A JP2948973B2 JP 2948973 B2 JP2948973 B2 JP 2948973B2 JP 4041622 A JP4041622 A JP 4041622A JP 4162292 A JP4162292 A JP 4162292A JP 2948973 B2 JP2948973 B2 JP 2948973B2
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- Prior art keywords
- molded body
- firing
- temperature
- weight
- thermal history
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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- Measuring Temperature Or Quantity Of Heat (AREA)
- Compositions Of Oxide Ceramics (AREA)
Description
【０００１】[0001]
【産業上の利用分野】本発明は、セラミックスなどの焼
成工程における熱履歴を検知するためのものであり、特
に陶磁器、ガラスセラミック、釉薬焼付けなどの１００
０〜１５００℃を超の温度域の焼成における熱履歴検知
用成形体に関する。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention is for detecting a heat history in a firing process for ceramics and the like, and particularly for detecting ceramics, glass ceramics, glazes and the like.
The present invention relates to a molded body for detecting heat history in firing in a temperature range of 0 to 1500 ° C or more.
【０００２】[0002]
【従来の技術】セラミックスの焼成工程において、温度
プロファイル、焼成炉の種類、炉内のセッティング等に
よって被焼成体の受ける熱履歴は変化する。即ち、焼成
温度が同じでも他の条件が異なれば熱履歴は異なること
となり、この熱履歴を正しく検知する必要があった。2. Description of the Related Art In the process of firing ceramics, the thermal history of the object to be fired changes depending on the temperature profile, the type of firing furnace, the settings in the furnace, and the like. That is, even if the firing temperature is the same, if other conditions are different, the thermal history will be different, and it is necessary to correctly detect the thermal history.
【０００３】例えば、実開昭５６−２９４４１号公報な
どに示されているゼーゲルコーンを用いて被焼成体の熱
履歴を検知することが行われていた。ゼーゲルコーンと
は、溶倒温度の異なる複数の三角錐状体を支持台上に備
えたものであり、このゼーゲルコーンを被焼成体と共に
焼成した後、各三角錐状体の倒れ方によって、熱履歴を
検知するようになっていた。しかし、これでは正確な検
知ができないことから、現在では使用されることが少な
くなっている。For example, the thermal history of a body to be fired has been detected using a Zegel cone disclosed in Japanese Utility Model Application Laid-Open No. 56-29441. A Zegel cone is one in which a plurality of triangular pyramids having different melting temperatures are provided on a support base.After firing this Zegel cone together with the object to be calcined, the thermal history is determined by the manner in which each triangular pyramid falls. Was to be detected. However, since accurate detection is not possible with this, it is rarely used at present.
【０００４】そこで、例えば特開平１−１８４３８８号
公報等に示されているように、セラミックスの未焼成成
形体を用いて、この成形体を被焼成体と共に焼成した
後、収縮による寸法変化を測定することによって、熱履
歴を検知することが行われていた。例えば、図３に示す
ようなリング状の成形体２０、あるいは図４に示すよう
なシート状の成形体３０が用いられていた。Therefore, as shown in, for example, Japanese Patent Application Laid-Open No. 1-184388, a green compact of ceramics is used, and the green compact is fired together with a body to be fired. By doing so, the thermal history has been detected. For example, a ring-shaped molded body 20 as shown in FIG. 3 or a sheet-shaped molded body 30 as shown in FIG. 4 has been used.
【０００５】なお、このような焼成収縮による寸法変化
を測定する場合、寸法変化は便宜的に温度に変換される
が、この温度は実温を測定したものではなく、熱履歴を
表すものであって、本発明では指示温度と呼ぶこととす
る。When such a dimensional change due to firing shrinkage is measured, the dimensional change is conveniently converted to a temperature. However, this temperature is not a measurement of the actual temperature, but a thermal history. Therefore, in the present invention, it is referred to as an indicated temperature.
【０００６】[0006]
【発明が解決しようとする課題】ところが、上記の熱履
歴検知用セラミックス成形体は、Ａｌ2 Ｏ3 −Ｓｉ
Ｏ2、またはＳｉＯ2 −ＭｇＯ系を主成分とし、多量の
不純物を含む天然原料からなるものであったため、焼成
収縮率にバラツキがあり、検知された指示温度の精度が
悪かった。However, the above ceramic molded body for detecting thermal history is made of Al 2 O 3 —Si.
Since it was made of a natural raw material containing O 2 or SiO 2 —MgO as a main component and containing a large amount of impurities, the firing shrinkage ratio varied, and the accuracy of the detected indicated temperature was poor.
【０００７】さらに、図３に示すリング状のものでは、
体積が大きいため、焼成炉内で広いスペースを必要と
し、図４に示すシート状のものでは、ソリが発生して正
しく寸法を測定できないなどの問題点があった。Further, in the ring-shaped one shown in FIG.
Since the volume is large, a large space is required in the firing furnace, and the sheet-shaped one shown in FIG. 4 has a problem that warpage occurs and dimensions cannot be measured correctly.
【０００８】[0008]
【課題を解決するための手段】そこで本発明は、４５重
量％以上のＳｉＯ2 と残部がＭｇＯ、ＣａＯなどからな
る主成分１００重量部に対し、ＢａＯを１〜１２重量部
添加してなる組成をもったセラミックス未焼成成形体を
熱履歴検知用成形体としたものである。Therefore, the present invention provides a composition comprising 1 to 12 parts by weight of BaO with respect to 100 parts by weight of a main component consisting of 45% by weight or more of SiO 2 and the balance being MgO, CaO or the like. The ceramic unsintered molded body having the above is used as a molded body for thermal history detection.
【０００９】本発明において、ＳｉＯ2 を４５重量％以
上としたのは、４５重量％未満では焼成時に変形を生じ
るためである。また、ＢａＯを添加する理由は、より低
温で収縮を可能にするためであり、ＢａＯの添加量が１
２重量部を超えると、焼成時に変形を伴い、熱履歴検知
用成形体としての機能を果たすことができないためであ
る。また、上記主成分中にはＳｉＯ2 の他に、５５重量
％以下のＭｇＯ、４５重量％以下のＣａＯを含んでもよ
く、さらに不可避不純物として、これらの他の成分を微
量に含んでいてもよい。In the present invention, the reason why the content of SiO 2 is set to 45% by weight or more is that if it is less than 45% by weight, deformation occurs during firing. The reason for adding BaO is to enable shrinkage at a lower temperature.
If the amount exceeds 2 parts by weight, deformation occurs during firing, and the function as a heat history detecting molded body cannot be achieved. In addition to the SiO 2 , the main component may contain 55 wt% or less of MgO or 45 wt% or less of CaO, and may further contain trace amounts of these other components as inevitable impurities. .
【００１０】[0010]
【実施例】以下本発明の実施例を説明する。Embodiments of the present invention will be described below.
【００１１】図１（ａ）（ｂ）に示すように、本発明の
熱履歴検知用成形体１０は、円板体に平行な弦部１２、
１２を形成したものであり、残された円弧部は優れた真
円度の測定面１１、１１としてある。また、表裏を区別
するためのドットあるいはアルファベットなどの刻印に
よる凹部１３が片面に形成され、上下面の角部には面取
り１４が施されている。As shown in FIGS. 1 (a) and 1 (b), a heat history detecting molded body 10 of the present invention has a chord portion 12 parallel to a disk body.
12 are formed, and the remaining arc portions are measurement surfaces 11 and 11 having excellent roundness. In addition, a concave portion 13 is formed on one side by engraving such as a dot or an alphabet for distinguishing the front and back sides, and a chamfer 14 is formed on the corners of the upper and lower surfaces.
【００１２】さらに、この成形体１０は、ＳｉＯ2 ４５
〜１００重量％、ＭｇＯ０〜５５重量％、ＣａＯ０〜４
５重量％からなる主成分１００重量部に対し、ＢａＯを
１〜１２重量％添加してなる組成からなっており、原料
粉末の粒径、成形体の生密度などを極めて厳密に管理
し、プレス成形してなる、未焼成成形体である。そし
て、後述するように、ある条件の下で焼成温度を変化さ
せて、この成形体１０の焼成後の寸法を測定し、寸法と
焼成温度の関係を換算表として用意しておく。その後、
異なる条件で焼成を行う際に、被焼成体と共にこの成形
体１０を焼成し、焼成後の寸法変化を測定することによ
って、上記換算表より指示温度を求めることができる。Further, the molded body 10 is made of SiO 2 45
-100% by weight, MgO0-55% by weight, CaO0-4
It has a composition in which 1 to 12% by weight of BaO is added to 100 parts by weight of a main component of 5% by weight, and the particle size of the raw material powder, the green density of the compact, and the like are extremely strictly controlled. It is a green compact formed by molding. As will be described later, the firing temperature is changed under certain conditions to measure the dimensions of the molded body 10 after firing, and the relationship between the dimensions and the firing temperature is prepared as a conversion table. afterwards,
When firing under different conditions, the molded body 10 is fired together with the object to be fired, and the indicated temperature can be determined from the above conversion table by measuring the dimensional change after firing.
【００１３】なお、前記したように、この指示温度と
は、実際の温度ではなく、熱履歴を便宜的に表したもの
である。即ち、本発明の熱履歴検知用成形体を用いれ
ば、焼成条件が異なる場合でも、指示温度を求めること
によって、熱履歴自体を管理することが可能となる。As described above, the indicated temperature is not an actual temperature but a heat history for convenience. That is, by using the heat history detecting molded body of the present invention, even when firing conditions are different, it is possible to manage the heat history itself by obtaining the indicated temperature.
【００１４】また、本発明の成形体は、さまざまな焼成
雰囲気の下で使用できるが、非酸化性雰囲気において
は、脱脂が不十分なことによるカーボンの発生があり、
また高温真空下においては、組成の一部が蒸発して凝縮
することがあり、不適当な場合があり得る。The molded article of the present invention can be used in various firing atmospheres. However, in a non-oxidizing atmosphere, carbon is generated due to insufficient degreasing.
Further, under a high-temperature vacuum, a part of the composition may evaporate and condense, which may be inappropriate.
【００１５】さらに、本発明の成形体１０は、弦部１
２、１２をもっていることから、図３に示した従来例に
比べて面積が小さく、焼成炉内で大きなスペースを必要
としない。なお、この弦部１２、１２は互いに平行でな
くてもよく、一ヶ所のみに形成してもよい。さらに、本
発明の成形体１０は、３〜１０ｍｍ程度の肉厚をもった
プレス成形品であるからソリなどが生じることはなく、
また寸法測定時には図１（ａ）に示すように、円弧をし
た測定面１１、１１間を定圧マイクロメータで測定すれ
ばよく、測定位置がずれても同じ直径Ｄを正確に測定で
きる。Further, the molded body 10 of the present invention has the chord 1
Since it has 2, 12, the area is smaller than that of the conventional example shown in FIG. 3, and a large space is not required in the firing furnace. Note that the chords 12 and 12 need not be parallel to each other, and may be formed only at one location. Furthermore, since the molded body 10 of the present invention is a press-molded article having a thickness of about 3 to 10 mm, no warpage or the like occurs,
Further, at the time of dimension measurement, as shown in FIG. 1 (a), the measurement between the arc-shaped measurement surfaces 11, 11 may be performed by a constant-pressure micrometer, and the same diameter D can be accurately measured even if the measurement position is shifted.
【００１６】また、本発明の成形体１０の形状について
は、密度が均一となるような単純な形状であれば、さま
ざまなものとすることができる。The shape of the molded body 10 of the present invention can be various as long as it is a simple shape having a uniform density.
【００１７】実験例１ ＳｉＯ2 、ＭｇＯ、ＣａＯ、ＢａＯを表１および図２に
示す組成とし、アルミナボールにより湿式粉砕し、レー
ザー光散乱法による粒度分析を行って、平均粒径３．０
±０．１μｍの範囲とした。この原料粉末に８．５重量
％のワックス系バインダーを添加混合し、噴霧乾燥する
ことによって、流動性の良い顆粒を得、この顆粒を、空
調された成形室にて、図１（ａ）（ｂ）に示す形状にプ
レス成形するが、このとき成形体の生密度を１．６００
±０．００５ｇ／ｃｍ3 の範囲内として、本発明の熱履
歴検知用成形体を得た。 Experimental Example 1 SiO 2 , MgO, CaO, and BaO were made into the compositions shown in Table 1 and FIG. 2, wet-pulverized with alumina balls, analyzed for particle size by a laser light scattering method, and found to have an average particle size of 3.0.
The range was ± 0.1 μm. 8.5 wt% of a wax-based binder was added to the raw material powder, mixed and spray-dried to obtain granules having good fluidity. The granules were placed in an air-conditioned molding room as shown in FIG. Press molding into the shape shown in b), where the green density of the molded body is 1.600.
Within the range of ± 0.005 g / cm 3 , a heat history detecting molded article of the present invention was obtained.
【００１８】これらの成形体を、１０５０℃で２時間、
１２５０℃で２時間、１４５０℃で２時間の３種類の条
件で焼成した。結果は表１に示す通りであった。[0018] These molded products were heated at 1050 ° C for 2 hours.
It baked on three conditions of 1250 degreeC for 2 hours and 1450 degreeC for 2 hours. The results were as shown in Table 1.
【００１９】[0019]
【表１】 [Table 1]
【００２０】表１より明らかに、ＳｉＯ2 が４５重量％
未満の場合は、焼成時にソリ変形を伴い、熱履歴検知用
成形体としての機能を果たすことができなかった。ま
た、ＢａＯを８重量％添加したＮｏ．６の組成では、１
０５０℃で１．１％、１２５０℃で１４．１％収縮し、
良好であったが、ＢａＯを１５重量％添加したＮｏ．９
の組成ではソリ変形のため不適当であることがわかっ
た。It is clear from Table 1 that the content of SiO 2 is 45% by weight.
If the ratio is less than the above range, warpage occurs during firing, and the molded article for detecting heat history cannot function. In addition, No. 8 containing 8% by weight of BaO was used. In the composition of 6, 1
Shrink 1.1% at 050 ° C, 14.1% at 1250 ° C,
Although it was good, No. 15 containing 15% by weight of BaO was used. 9
The composition was found to be unsuitable due to warpage deformation.
【００２１】実験例２ 実験例１と全く同様にして、表１中Ｎｏ．２の組成で、
直径Ｄが２２．３００ｍｍの熱履歴検知用成形体１０を
用意した。この成形体１０を厳密に管理校正された焼成
炉を用いて、酸化雰囲気にて、昇温速度２００℃／時、
最高焼成温度で２時間保持、降温速度３００℃／時とし
て焼成し、３５０℃で１時間脱脂した。焼成後の成形体
１０の寸法を、２０℃にて定圧マイクロメータで測定し
た。 Experimental Example 2 In the same manner as in Experimental Example 1, Table 1 With the composition of 2,
A heat history detecting molded body 10 having a diameter D of 22.300 mm was prepared. The molded body 10 was heated in an oxidizing atmosphere at a rate of 200 ° C./hour in a sintering furnace strictly controlled and calibrated.
It was held at the highest firing temperature for 2 hours, fired at a temperature lowering rate of 300 ° C./hour, and degreased at 350 ° C. for 1 hour. The dimensions of the molded body 10 after firing were measured at 20 ° C. with a constant pressure micrometer.
【００２２】焼成温度（指示温度）をさまざまに変化さ
せて、それぞれ２０個の成形体１０の焼成の焼成を３回
繰り返して行った。この結果は、表２および図５に示す
通りである。By varying the firing temperature (instruction temperature) in various ways, firing of each of the 20 compacts 10 was repeated three times. The results are as shown in Table 2 and FIG.
【００２３】また、各温度における、寸法のばらつき
（３σ）と、その温度での１℃当たりの寸法変化量（接
線の傾き）から、 指示温度の検知精度＝±寸法のばらつき／１℃当たりの
寸法変化量 により、指示温度の検知精度（３σ）を算出した。結果
は、表２に示す通り、１１００〜１３００℃の範囲内
で、指示温度の検知精度を±２℃以内とすることができ
た。Further, from the dimensional variation (3σ) at each temperature and the dimensional change per 1 ° C. (tangent slope) at that temperature, the detection accuracy of the indicated temperature = ± the dimensional variation / per 1 ° C. The detection accuracy of the indicated temperature (3σ) was calculated from the dimensional change. As shown in Table 2, the detection accuracy of the indicated temperature was within ± 2 ° C. within the range of 1100 to 1300 ° C.
【００２４】さらに、表２では指示温度５０℃ごとの成
形体の寸法を示しているが、もっと細かな指示温度ごと
の寸法を測定しておくことによって、成形体の寸法と指
示温度の換算表とすることができる。Further, Table 2 shows the dimensions of the compact at each indicated temperature of 50 ° C. By measuring the dimensions more precisely at each designated temperature, a conversion table of the dimensions of the compact and the designated temperature is obtained. It can be.
【００２５】[0025]
【表２】 [Table 2]
【００２６】また、上記実施例では、熱履歴検知用成形
体１０を得るために、原料の粒径３．０±０．１μｍ、
成形体の生密度１．６００±０．００５ｇ／ｃｍ3 とし
たが、いずれもこの値に限定されるものではなく、さま
ざまに変化させることができる。通常、粒径については
±０．１μｍで管理し、生密度については±０．００５
ｇ／ｃｍ3 の範囲内にバラツキを押さえれば、指示温度
の検知精度を±２℃とすることが可能であった。In the above embodiment, in order to obtain the heat history detecting molded body 10, the raw material has a particle size of 3.0 ± 0.1 μm,
Although the green density of the molded body was 1.600 ± 0.005 g / cm 3 , none of these values is limited to this value, and various changes can be made. Usually, the particle size is controlled at ± 0.1 μm, and the green density is ± 0.005.
If the variation was kept within the range of g / cm 3 , the detection accuracy of the indicated temperature could be made ± 2 ° C.
【００２７】[0027]
【発明の効果】このように本発明によれば、４５重量％
以上のＳｉＯ2 にＭｇＯ、ＣａＯなどを含む１００重量
部に対し、ＢａＯを１〜１２重量％添加してなる組成を
もったセラミックス未焼成成形体を熱履歴検知用成形体
としたことによって、指示温度の測定精度を±２℃以内
と極めて高精度にできることから、焼成条件が変わって
も焼成工程を厳密に管理することができ、優れた焼結体
を得ることが可能となる。また、特に１５００℃以下の
低温域での焼成管理を可能とすることができる。As described above, according to the present invention, 45% by weight
More MgO to SiO 2, relative to 100 parts by weight, including CaO, by the ceramic green shaped body having a composition obtained by adding BaO 1 to 12 wt% and the thermal history detection moldings, instruction Since the measurement accuracy of the temperature can be made extremely high within ± 2 ° C., the firing step can be strictly controlled even if the firing conditions are changed, and an excellent sintered body can be obtained. In addition, it is possible to control firing in a low temperature range of 1500 ° C. or less.
【００２８】[0028]
【図１】（ａ）は本発明実施例の熱履歴検知用成形体を
示す平面図、（ｂ）は同図（ａ）中のＸ−Ｘ線断面図で
ある。FIG. 1A is a plan view showing a heat history detecting molded body according to an embodiment of the present invention, and FIG. 1B is a cross-sectional view taken along line XX in FIG. 1A.
【図２】本発明の熱履歴検知用成形体の主成分であるＳ
ｉＯ2 −ＭｇＯ−ＣａＯの組成範囲を示す三成分組成図
である。FIG. 2 shows S which is a main component of the heat history detecting molded body of the present invention.
FIG. 3 is a ternary composition diagram showing a composition range of iO 2 —MgO—CaO.
【図３】従来の熱履歴検知用成形体を示す斜視図であ
る。FIG. 3 is a perspective view showing a conventional heat history detecting molded body.
【図４】従来の熱履歴検知用成形体を示す斜視図であ
る。FIG. 4 is a perspective view showing a conventional heat history detecting molded body.
【図５】本発明の熱履歴検知用成形体における、焼成収
縮率と指示温度の関係を示すグラフである。FIG. 5 is a graph showing the relationship between the firing shrinkage and the indicated temperature in the molded article for heat history detection of the present invention.
１０・・・熱履歴検知用成形体 １１・・・測定面 １２・・・弦部 １３・・・凹部 １４・・・面取り DESCRIPTION OF SYMBOLS 10 ... Heat history detection molded body 11 ... Measurement surface 12 ... String part 13 ... Depression 14 ... Chamfer
───────────────────────────────────────────────────── フロントページの続き (56)参考文献 特開 平１−184388（ＪＰ，Ａ) 特開 昭63−11563（ＪＰ，Ａ) 特開 平５−1955（ＪＰ，Ａ) 実開 昭56−29441（ＪＰ，Ｕ) (58)調査した分野(Int.Cl.6，ＤＢ名) G01K 11/00 G01K 5/48 ──────────────────────────────────────────────────続 き Continuation of the front page (56) References JP-A-1-184388 (JP, A) JP-A-63-11563 (JP, A) JP-A-5-1955 (JP, A) 29441 (JP, U) (58) Fields investigated (Int. Cl. 6 , DB name) G01K 11/00 G01K 5/48
Claims (1)
Ｏなどを含む１００重量部に対し、１〜１２重量部のＢ
ａＯを添加した組成のセラミックス未焼成成形体からな
ることを特徴とする熱履歴検知用成形体。1. A 45 wt% or more MgO to SiO 2, Ca
1 to 12 parts by weight of B with respect to 100 parts by weight including O
A molded article for thermal history detection, comprising a ceramic unsintered molded article having a composition to which aO is added.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP4041622A JP2948973B2 (en) | 1992-02-27 | 1992-02-27 | Molded body for thermal history detection |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP4041622A JP2948973B2 (en) | 1992-02-27 | 1992-02-27 | Molded body for thermal history detection |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH05240716A JPH05240716A (en) | 1993-09-17 |
| JP2948973B2 true JP2948973B2 (en) | 1999-09-13 |
Family
ID=12613434
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP4041622A Expired - Lifetime JP2948973B2 (en) | 1992-02-27 | 1992-02-27 | Molded body for thermal history detection |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP2948973B2 (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110411228A (en) * | 2019-07-30 | 2019-11-05 | 上海富驰高科技股份有限公司 | Vacuum drying oven furnace temperature equal control method in sintering process |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP4762092B2 (en) * | 2006-09-07 | 2011-08-31 | 京セラ株式会社 | Thermal history sensor |
-
1992
- 1992-02-27 JP JP4041622A patent/JP2948973B2/en not_active Expired - Lifetime
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110411228A (en) * | 2019-07-30 | 2019-11-05 | 上海富驰高科技股份有限公司 | Vacuum drying oven furnace temperature equal control method in sintering process |
Also Published As
| Publication number | Publication date |
|---|---|
| JPH05240716A (en) | 1993-09-17 |
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